Manufacture of by-products from distillery-slop.



Amman. v'oN LAszLorFY, or PEORIA, ILLINOIS.

MANUFACTURE OF BY-PRODU'GTS FROM DISTILLERY-SLOR- No Drawing.

To'all whom it may concern:

Be it known that I, ALADAR VON Lzisz- LOFFY, subject of Francis Joseph, King of Hungary, residing at Peoria, in the county of Peoria and State of Illinois, have invented certain new and useful Improvements in the Manufacture of By-Products from Distillery-Slop; and I do-hereby declare that the following is a full, clear, and exact descripgroups of by-products.

Anobject of the invention is to separate the mixture of substances represented in dis. tillery slop into solutions containing glycsoluble nitrogenous substances, salts etc.

Anotherobject of the invention is to carry 1 out the separation of solutions from consuspended solids.

centrat'ed slop by a solvent without the ad dition of substances that would be hurtful to any of theproducts.

Another object of the invention is to sepa- -rate the mixture of substances represented in distillery slop into solutions containing the named substances without destroying the value of the slop as a feed, and without diminishing its commercial value as a concentrated cattle-feed. 1 Another objectjs to extract said solutions from slop without destroyingthe feed value of the same whereby the s'lops can be made to yield greater returns in money value than produced alone bythe slop as aiEeedQ Still another object of the inventionjs the recovery of any certain by-product or by-products, contained-in the slop without destroying others contained therein. This process is intended for the heat ment of slop used as a feed, especially gra'in,potato, or sugar-beet slop, but it can also be used for the slop or vinassede rived from other raw materials.

Distillery slop consists of a solution and The solution contains soluble nitrogenous matter,; carbohydrates,

gums, salts,'lactic and succinic acids, glyc: erm and other substances. Vanous processes' have been devised for extracting by-p'rod Specification of Letters Patent. 1

l Patented July 2'3, 1915.

Application filed January 30, 1911; Serial No. 605,611.

ucts, especially glycerin, from the slop and in some of those processes the slop is treated with alcohol in order to obtain sald glyc 'erin, but the practice'is such that in order to obtain the by-products either the whole slop or the dissolved substances of the same are sacrificed and made unfit for a feed. The slop is of such value as a feed, especially in the case of grain-slop, that the value of the by-products obtained from it by the older methods ,is not sufiicient to warrant destruction of the feed-value even if the solids are removedbefore the process of extraction begins.

One of the objects of the'invention', therefore, and a very importantone, is to pro I vide a process by which the dissolved substances contained in the slop can be economically separated into a solid part containin erin, lactic acid, succ1n1cac1d,.fats, gums,

almost all the substances valuable as a fee and solution containing the glycerin, the

lactic acid and the succinic acid'of the slopsolutionin a highly concentrated state and without destroying the value of any of the original slop for a feed.

I obtain this separation preferably by concentrating the slop through evaporation,

to a syrupy or a pasty consistency, driving off the largest part of the water, afterward treating the material left with alcohol. The

alcohol precipitates most of the albumens,"

.essary to separate the by-products from each other. And by first separating the .7

slop with the aid of alcoholinto a feed part and into a solution containing the by-products, the chemicals necessary forobtaining the latter will not come in contactwith the substances of the-slop which are valuable as a feed. This solution must not be regarded as amixture containing the named sub- 7 stances only, since there are always nitrogenous substances, small amounts of salts, etc.,

7 an alco-. a

i "holic solvent, does not necessarlly contam lactic and succinic acids. Their presence .depends upon the treatment the slop receives before itis mixed with the alcoholic solvent. For instance, by'neutralizing the slop or by transforming the said acids into v salts, which are insoluble in the solvent used,

a solution is obtained which contains, together with other substances, glycerin and fat but no acids. Therefore, my process need not necessarily carry with it the si multaneous extraction of the acids and glycerin. I have found that it is both technically and commercially advantageous to treat with the alcoholic solvent without first neutralizing the slop.

By proceeding in the manner described two very important advantages are gained the soluble substances of the slop-are at once divided into a concentrated mixture of lactic. acid, succinic acid, glycerin and fat,..and into substances valuable as a feed, and a further advantage is that the quality of the feed-residue is not depreciated by the presence of chemicals.

The alcohol not only divides the,slop into a soluble and insoluble part but it also leaves I the insoluble part in such a physical conthe invention, -a more detailed explanation dition that the mechanical separation of the solids and the solution can be-accomplished with the greatest ease, for instance either bysettling or filtration. Moreover, the physical condition of the residue of the alcohol separation is such that other by-prod ucts can be separated from it such, for instance, as gums, dextrins, soluble albumens,

etc., and in this specification the separation of the slop into a solution containing glycerin, organic acids, fats, etc., and into'a solid part containing the feed part of the slop, gums, etc., will be referred to as an alcohol-separation. 4 I recover the alcohol used for separation by distilling the same off in an alcohol distilling apparatus which will eliminate the water absorbed by the alcohol. f In order to simplify and make clear the explanation of my invention, I desire to state at'this time that wherever, in any stage of the process, the recovery of the alcohol or other solvent used in this process is not especially mentioned it isunderstobdthat this recovery takes place, for economical reason particularly, in any style of distilling or rectifying apparatus for this pur-.

pose.

Having now explained the principles of of the manner of making use of these princip1es,will be given; 1

- The practice may includedifierent methodsz-For example, by boiling down the slop as itcomes from the still, hulls and all, preferably in vacuum, until the largest part of the water is removed andthen treating it with alcohol, or by separating the suspended solids from the aqueous solution of the slop by settling, filtering or by the use of a centrifugal machine, boiling the aqueous solution down to'the consistency of athick syrup preferably in vacuum, and using only the syrup, which contains the largest part of the glycerin, organic acids, gums, and some fat of the slop, for the alcohol separation. Or, again I can separate the suspended solids of the slop by mechanical means,

boil the thus obtained aqueous solution to alcohol. Losses of lactic acid and glycerin which are unavoidable in drying are prac tically eliminated. The material can be easilyhandled, the loss of solvent is very small, and the solvent can be easily recovered.

The removal of the water from the slop before treating the same with alcohol is not an absolute necessity, but more practical. But preferably the alcohol is gradually added to the slop which has been concentrated to a syrupy consistency. This gradual addition of the alcohol allows the [slop -to'become thoroughly mixed with itandv 'when a certain percentage of the latter in themixture'is reached the coagulation of the insoluble substances is in finer particles and the extraction of the soluble substances more complete. KI can also make the alcoholseparation a cont nuous one byrunnmg a contmuous stream of concentrated slop and alcohol into a mixing vessel wherefrom I can continuously separate the precipitated solids by mechanical means from the solution, and d1st1ll the alcohol out of said solutlon in a continuous manner, and in a continuous manner, also, eliminate the alcohol' from'the se -arated solids.

referably I use for the alcohol-sep aration,

ethyl-alcohol, but I can use'methyl alcohol or alcohol to which other substances have been added eitlfer as denaturingagents or in order to make certain impurities insoluble in the alcohol. In the latter case I can use either ethyl-alcohol,methyl-alcohol or mixture. of either or both with ethyl-' ether, fusel-oil, other alcohols, chloroform, ,tetrachlorid of carbon and other such mixtures which the alcohol will predominate.

, order to simplify the claims and make them more easily understood I use the term alcoholic solvent meaning alcohols as well as the mixtu as just enumerated. In the claims, also, wen the terms alcohol-water mixture or alcohol and water is used they will be taken to mean alcohol mixed withwater.

, The alcohol used for the alcohol separation as well as the mixtures named above can be used at any temperature cold or hot,

but preferably I use the hot alcohol in the treatment of the whole slop in order to more easily separate the fats, and in' order to obtain the glycerin and the organic acids in a state ofhigher purity I can repeat the alcohol treatment for further separation, proceeding, for example, in the following I manner: recovering the alcohol from the solution resulting from the first alcohol-separation and then boiling such solution until it has a thick syrupylconsistency. Now strong alcohol isagain added to obtain a new precipitation of impurities which are eliminated by filtering exactly in the same way as in the first instance and preferably in the latter case ethyl-ether of fusel-oil is added to the alcohol.

It has already been stated that the physical condition of the residue of the alcohol separation is such that other byproducts can be separated "from the same as for instance, the gums, soluble albumens,salts, etc.

The separation of these substances from the feed part is made more easy by reason of the fact that some of them are found to be soluble in alcohol-water mixtures of a certain strength and this treatment of the residue with gradually weaker solutions of alcohol is an important feature of my invention and admits of separating a variety of diiferent substances'from the slop. For

example, by adding water to the residue of the alcohol-separation, which naturally contains a large percentage of alcohol I can get practically all of the gums in solution and after recovering the alcohol and evaporating the water the gums areleft.

Finally, the treatment of the residue is to be explained. As can bereadily-seen from the foregoing, the methods employed in obtaining this residue are such that the said residue is in no way depreciated as a commercial cattle-feed.

No injurious chemicals whatsoever have been used and the residue is made to contain a largenproportion of the true protein-substances bythe separation of the by-produc'ts enumerated, and this is a very important advantage indeed. But still another advantage is derived by eliminating the organic acids, -the glycerin 'and other substances from the syrupy slop since the latter then loses its sticky and gummy character. The concentrated liquid part of the slop reduced to a syrup cannot be successfully dried until" the 0 organic acids and the glycerin, etc., are extracted by the present process. The residue of extraction is"; therefore either dried alone or by its admixture with absorbent nllaterial, for instance, the solid part of the s op.

The following is an example of the preferred mode of practising my invention.

alcohol of 190 proof. The concentrated slop is thoroughly mixed with the alcohol and after a few minutes'the coagulation of the substance insoluble in alcohol takes place. I run the mixture now into a second closed .tub provided with a perforated false bottom and the alcohol solution is allowed to filter out. After the flow of the-alcoholic solution has ceased I Wash the residue with 800 gallons of alcohol which is added to the solution just run ofl.

The solution thus obtained is now run into a distilling apparatus and after the alcohol is distilled hit, a thicksyrup is left representing a concentrated solution of glycerin and organic acids together with a percentage of fat and impurities. The treatment of this syrup will be described later attention being directed at this time to treatment of the resi due of thealcohol-separationleft in the tub.

[This naturally contains much alcohol and the gums are obtained in solution by adding enough watertobring the total volume up to 1250 gallons. This alcohol-Water solution is filtered from the insolubles, freed from alcohol, and boiled down in vacuum. The residue of the boiling represents the gums deamount .of dextrins. This extraction with an alcohol-water mixture can be repeated andfinally the alcohol is driven out of the residue representing the feed part which later is mixed with the cakes which were ob tained by. running the original slop through the filter-presses, and this mixture of the solids of the original slop, and the said residue,

' rived from the grain together with a certain is dried and used as an unimpaired'cattlefeed. v I

The concentrated mixture ofby-products contains lactic acid, succinic acid, glycerin, fat, some salts and impurities such as salts andnitrogenou's substanc'esas already explained. The fat easily separates from this mixture and'canbe skimmedoff. The re.- maining mixtureof byfproducts may be recontaining a lieved of the largest part of the impurities by adding to it a mixture of alcohol and ether. By doing so more salts and nitrogenous substances are precipitated from the mixture of by-products. The remaining solution is drawn ofi from the insoluble part and again concentrated. The separation of the resulting mixture of by-products does not constitute a part of the present application but forms the subject of a divisional feed and leaves the feed-residue richerm and containing a higher percentage of the most valuable feedsubstances-the proteins.

The total value of by-products extracted and of the feed recovered is far in excess of the values that can be obtained by any older processes.

Having thus claim 2- I 1. The process of precipitating albumenous and gummy substances from undried distillery material, consisting in treating said material with an alcoholic solvent, and separating the solution resulting from such treatment from theinsoluble part. a

2. The process of recovering by-products from distillery refuse which consists in preparing from said refuse a concentrated material containing the by-products in an undried state, treating said material with an alcoholic solvent, and separating the solution resulting from this treatment from the insoluble part. p I

3. The process of recovering a solution containing'a plurality of by-products from dis tillery-slop, consisting in evaporating slop to a syrupy consistency, mixing it afterward with an alcoholic solvent, and separating the solution of by-products resulting from this treatment from the insoluble part.

4.-,The process of recovering a solution containing a plurality of by-products and a feed from distillery-slop, consisting in evaporating slop to a syrupy consistency, mixing with the same analcoholic solvent, separating the solution resulting from this treatment ing the solvent.

Theyprocess of recovering a solution' plurality of by-products and .a feed from a mixture of substances derived from distillery-slop, consisting in treating said mixture of substances in 9.

described my invention, Iv

from the insoluble part, and recover-- concentrated state with an alcoholic solvent, separating the solution resulting. from this treatment from the insoluble part, andrecovering the solvent.

6. The process of separating a mixture of substances derived from distillery'slop into a-feed and a solution containing lactic acid; succinic acid, glycerin and fat, consisting in treating said mixture of substances in a concentrated state, with an, alcoholic solvent,

treatment-from the residue, and recovering the solvent from the residue.

7. The process of separating the substances dissolved in distillery-glgp into feed and into a solution containing lactic acid, succinic acid, glycerin and fat, consisting in separating slop into treating this part afterward with an alcoholic solvent, separating the solution thus obtained from the residue, and recovering the solvent from the residue.

v a solid part and a liquid part, removing water from the liquid part,

8. The process of separating the sub-,,.

stances dissolved in distillery-slop into feed and into a solution containing lactic acid,

succinic acid, glycerin and fat, consisting in separating slop into a solid part and into a liquid part, removing water from the liquid part, treating this part afterward with an slop into a solid residue and a solution con- 7 taining lactic acid, succinic acid, glycerin, and fat, consisting in evaporating slop to a syrupy consistency, mixing the latter with an alcoholic solvent, separating the alcoholic solution from the residue, and recovering the solvent from the residue.

11. The process of separating from distillery-slop gums, dextrins, nitrogenous substances and salts and a feed, consisting in removing water from slop, treating the same with an alcoholic solvent, separating the solution thus obtained from the residue, treating the residue with alcohol-water-mixtures, and separating the alcohol-water-solution from the residue.

12. The process ofseparating from distilgums, dextrins, nitrogenous sublery-slop and salts and a feed consisting in stances,

removing water from slop, treating the same 75 separating the solutionresultingffrom this i separating said mixture of substances into a with an alcoholic solvent, separating the 'so-' lution thus obtained from the residue, treating the residue with alcohol-water mixtures, separating the alcohol-water-solution from the residue, and treating the residue with Water. i

13. The process of separating from distillery-slop, gums, dextrins, nitrogenous substances and salts and a feed, consisting .in removing water from slop treating the. same with an alcoholic solvent, separating the solution thus obtained from the residue, treat- ,ing the residue with water, and separating the new solution from the residue. I

14. The process of separating from the liquid part of distillery-slop gums, dextrins nitrogenous substances and salts and a feed, consisting in separating slop into a solid part and a liquid part, evaporating the liquid part to a syrupy consistency, treating the liquid part afterward with an alcoholic solvent, separating the solution thus obtained from the residue, treating the'residue with alcohol-water-mixtures, and separating the alcohol-water solution from the residue.

15. The process of recovering a solution containing lactic acid, succinic acid, glycerin, soluble nitrogenous substances, salts and fat, and. another solution containing gums, dextrins, nitrogenous substances, salts, and a feed from a mixture of substances derived from distillery slop, consisting' in treating said mixture of substances with an alcoholic-solvent thereby solution containing'lactic acid, succinic acid glycerin, fat, nitrogenous substances and salts" soluble in said-solvent,- and a residue,

treating the residue with alcohol-water-mixtures thereby separating said residue into a solution containing gums, dextrins, soluble nitrogenoussubstances and salts, and into a new residue, and recovering the solvent from .the new residue.

16. In the process of recovering a plurality of by-products from distillery-slop, the

process which consists in removing Water a from slop, treating the latter with'an alcoholic solvent, separating the solution thus obtained from the residue concentrating the solution by evaporating the solvent, treating the resulting mixture of by-products with an alcoholic solvent, and separating this solution from the new residue.

17. The process of separating a mixture of substances'derived from distillery-slop into a plurality of groups of by-products,

consisting in mixing said substances with an alcoholic solvent in a continuous manner, and separating the resulting solution from the insoluble residue in a continuous manner.

18. The process of recovering by-products' from distillery-refuse which. consists in pre- ALADAR vo LAsZLOFFY. Witnesses: q

CHAS. B. MGDOUGAL,

A. Bunxmmm'. 

